Process for preparation of chlorine nitrate

ABSTRACT

A NOVEL PREPARATION OF CHLORINE NITRATE BY REACTING FNO2 AND CA(OCL)2.

Unite d States Patent Office 3,798,312 Patented Mar. 19, 1974 3,798,312 PROCESS FOR PREPARATION OF CHLORINE NITRATE Donald Pilipovich, Agoura, Calif., and Charles B. Lindahl, Sand Springs, Okla., assignors to the United States of America as represented by the Secretary of the Navy No Drawing. Filed Sept. 24, 1971, Ser. No. 183,651 Int. Cl. C01]: 21/20, 21/52; Ctllf 11/22 US. Cl. 423386 3 Claims ABSTRACT OF THE DISCLOSURE A novel preparation of chlorine nitrate by reacting FNO and Ca(OCl) BACKGROUND OF THE INVENTION (1) Field of the invention This invention relates to a new method of preparing chlorine nitrate.

(2) Description of the prior art It is well known that ClNO is an important compound which may be used in the synthesis of numerous other inorganic compounds.

Chlorine nitrate has previously been prepared by reaction of either C1 or C10 with N0 or N 0 and by reaction of ClF with HNO as shown in Pat. No. 3,472,- 635. The synthesis using the explosive chlorine oxides are associated with a definite hazard potential while the CIF method requires separation of ClNO from its by-product HF where the boiling points differ by only a few degrees temperature. In view of such difliculties a new route was sought obviating the use of a halogen fluoride.

SUMMARY OF THE INVENTION The present concept involves a novel method of preparing chlorine nitrate by reacting nitryl fluoride with calcium hypochlorite. Thus a novel method of preparing chlorine nitrate, a valuable compound from which other inorganic compounds may be prepared, is added to the deficient and unsatisfactory literature on such synthesis.

OBJECTS OF THE INVENTION Accordingly an object of the invention is to provide a novel process for the preparation of chlorine nitrate.

Another object of the invention is to provide a method for preparing chlorine nitrate which obviates the use of a halogen fluoride.

Still another object is to provide a method for preparing chlorine nitrate which is rapid, convenient and produces chlorine nitrate of high purity.

Other objects, advantages and novel features of the invention will become apparent from the following detailed description of the invention.

DESCRIPTION OF THE PREFERRED EMBODIMENT This invention comprises a novel process of preparing chlorine nitrate by reacting nitryl fluoride with calcium hypochlorite. The reaction equation is:

The reaction may occur over a wide variety of reaction temperatures, FNO pressures, reactant ratios and Ca(OCl) purities. Reactions have produced ClN0 at temperatures from 78 C. to ambient using both 95% research grade Ca(OCl) and 70% grade Ca(OCl) Pressures of FNO have ranged from 0 at end of the reaction to initial pressures of 120 p.s.i. Reactant ratios have varied from slight excesses of FNO to 15 fold excesses of Ca(OCl) and reaction times have ranged from less than one hour to about 2 days.

Chlorine nitrate has many utilities but is primarily used as a starting compound for other inorganic compounds including metal nitrates which have established utilities. For example, Co(NO and Mn(NO are both prepared from ClNO and are extensively used to prepare electrodes used in O-depolarized primary cells. Additionally, Ti(NO is prepared from ClNO which is used in coating and annealing processes for magnetic materials.

EXAMPLE Two grams of untreated commercial grade Ca(OCl) (approximately 10 mmoles of Ca(OCl) were placed in an unpassivated 30 ml. stainless steel cylinder. This was evacuated, to remove gaseous substances, and 2.54 mmoles of FNO were condensed in at -196 C. The reactor was stored for 44 hours at about -60 C. Subsequent fractional condensation of the sample produced 2.29 mmoles of ClNO which gives a 90.2% yield (2.29 mmoles) based on the FNO added.

Thus a novel low-cost, one-step ClNO preparation is formulated with easy separation of the ClNO from the solid CaF byproduct.

Obviously, many modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described.

We claim:

1. The process for producing ClNO which comprises:

reacting calcium hypochlorite with nitryl fluoride according to the following equation:

Ca(OCl) +2FNO CaF +2ClNO With the reaction temperature ranging between 78 C. to ambient temperature and separating the ClNO; from the solid CaF by product.

2. The process for producing ClNO in claim 1 wherethe pressures of FNO range from p.s.i. at the beginning of the reaction to 0 p.s.i. at the end of the reaction; reaction ratios vary from slight excesses of FNO to 15 fold excesses of Ca(OCl) and reaction times range from about one hour to about two days.

3. The process for producing ClNO which comprises: placing 10 mmoles of Ca(OCl in a reactor cylinder; evaculating said cylinder to remove gaseous substances; condensing 2.54 mmoles of FNO in said reactor cylinder at -196 C.; holding the reactor cylinder for 44 hours at about --60 0.; wherein subsequent mmoles of C1NO fractionation produced 2.29

References Cited UNITED STATES PATENTS 3,472,635 10/1969 Schack.

OSCAR R. VERTIZ, Primary Examiner H. S. MILLER, Assistant Examiner US. Cl. X.R. 423-490 

